CN106730040A - 具有bmp/pla缓释涂层的种植体活性表面 - Google Patents

具有bmp/pla缓释涂层的种植体活性表面 Download PDF

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CN106730040A
CN106730040A CN201611207441.4A CN201611207441A CN106730040A CN 106730040 A CN106730040 A CN 106730040A CN 201611207441 A CN201611207441 A CN 201611207441A CN 106730040 A CN106730040 A CN 106730040A
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pla
planting body
bmp
active surface
titanium
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刘宇
张久文
蔡俊江
彭鹏
李闪
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Dalian Sansheng Science & Technology Development Co Ltd
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Abstract

本发明公开了一种具有BMP/PLA缓释涂层的种植体活性表面，所述种植体外表面具有钛基底层，所述钛基底层外表面具有二氧化钛基层，所述二氧化钛基层上涂覆有BMP/PLA复合涂层。将打磨清洗好的种植体表面用75μm TiO2颗粒喷砂后在酸蚀剂中进行表面酸刻蚀处理，再经碱热处理后依次涂覆PLA和BMP‑2。本发明的方法有效提高了种植体表面的粗糙度和表面能，增强材料表面的活性，增加了BMP蛋白的载荷量和聚乳酸与种植体表面的结合强度，同时利用聚乳酸的支架性能，构建BMP/PLA涂层，通过PLA自身降解调节BMP‑2的缓慢释放，促进种植体与周围骨组织的早期骨愈合。

Description

具有BMP/PLA缓释涂层的种植体活性表面
技术领域
本发明属于生物医用植入物领域，具体涉及一种具有BMP/PLA缓释涂层的种植体活性表面及其构建方法。
背景技术
钛金属具有良好的生物相容性、力学性能和机械加工潜力等优点，目前作为牙种植材料在口腔科广泛应用。然而，钛本身具有生物惰性，被植入机体后，引发愈合时间长、生物活性低，诱导骨修复能力差等问题。为了提高其生物活性，目前大多采用等离子喷涂、离子溅射、电泳、微波烧结等技术改造种植体表面的微观物理形貌和化学成分，形成具有较好生物相容性的粗糙多孔表面，并提高了种植体育骨组织的结合强度，但此类种植体与骨组织之间仍然是物理性结合，但无骨诱导性能，与周围组织的生物相容性低，临床上口腔种植治疗的周期相当长，给患者的生活带来诸多不便。近年来，在改造种植体表面的微观物理形貌的基础上，在其表面制备或涂覆生物活性分子涂层或薄膜，达到促进成骨细胞的增殖和分化来促使新骨的形成，缩短了治疗周期。
骨形态发生蛋白(BMP)为高效骨诱导因子，可在骨修复早期通过诱导未分化间充质细胞和骨髓基质细胞不可逆分化为软骨细胞和成骨细胞而诱导新骨形成。目前，将BMP作为生物活性分子引入种植体表面的研究很多，但由于BMP吸附的量很有限，在生理条件下短时间内被快速释放或吸收降解，因此无法在局部发挥持续剌激和诱导成骨的作用，其生物活性难以得到充分发挥。
发明内容
鉴于上述现有技术中存在的问题，本发明的目的在于提供一种具有BMP/PLA缓释复合涂层的种植体活性表面及其构建方法。
本发明的技术方案如下：
一种具有BMP/PLA缓释复合涂层的种植体活性表面，其特征在于，所述种植体外表面具有钛基底层，所述钛基底层外表面具有二氧化钛基层，所述二氧化钛基层的外表面涂覆有BMP/PLA复合涂层。
在上述技术方案中，所述的具有BMP/PLA缓释复合涂层的种植体活性表面，其制备方法包括以下步骤：
(1)将钛金属种植体表面用200、300、600和2000目砂纸逐级打磨，清洗，在60℃烘干；
(2)用75μmTiO2颗粒，通过喷嘴对种植体表面进行喷砂处理；
(3)将喷砂处理后的种植体置于氢氟酸与盐酸组成的混合酸蚀剂中进行表面刻蚀处理，取出种植体超声清洗，室温自然干燥；
(4)将进行表面刻蚀处理、干燥后的种植体置于60℃、5mol/L NaOH溶液孵育24-48h，用水超声清洗后，干燥后600℃下处理1-2h；
(5)将高温处理后的种植体在紫外线下消毒24-48h；
(6)将聚乳酸溶于CH3Cl3，加入蒸馏水制成乳化液，将步骤(5)中紫外线消毒好的种植体，在无菌条件下浸入聚乳酸乳化液中，置于通风处蒸发水和溶剂，重复上述操作数次，得聚乳酸涂层种植体；
(7)聚乳酸涂层种植体浸入1-3mg/mL BMP-2溶液中，在4℃下放置24-48h，真空冷冻干燥。
进一步地，在本发明的上述技术方案中，在步骤(2)中，所述的喷砂处理条件为：压缩空气压力为0.3-0.4MPa，喷嘴离种植体表面的距离为5-10cm，喷射时间为2-10s。
进一步地，在本发明的上述技术方案中，在步骤(3)中，所述的混合酸蚀剂为47％的氢氟酸与38％的盐酸以体积比1:1混合的混合液
进一步地，在本发明的上述技术方案中，在步骤(3)中，所述的表面刻蚀处理温度为60℃，刻蚀处理时间为10-20min。
进一步地，在本发明的上述技术方案中，在步骤(7)中，每隔12小时换BMP-2溶液一次。
进一步地，在本发明的上述技术方案中，所述BMP-2溶液的制备步骤为：将BMP-2溶解于pH值为7.0的PBS或溶解于SBF溶液中。
聚乳酸(polylacticacid，PLA)为一种重要聚酯类可生物降解高分子聚合物，其主链含有不稳定易被水解或酶解的化学键，从而能在生物体内水解脱酯，生成乳酸单体，在体内乳酸脱氢酶的作用下生成丙酮酸，作为能量代谢物质参与三羧酸循环，终产物为Н2О和СО2，经肺、肾、皮肤排泄。聚乳酸具有良好的机械性能和生物相容性，其三维多孔结构和可生物降解性使其成为BMP等生长因子的重要缓释支架材料
本发明结合采用多种表面处理技术，对种植体的钛金属表面进行表面处理，有效提高了种植体表面的粗糙度和表面能，增强材料表面的活性，增加了BMP蛋白的载荷量和聚乳酸对表面的结合强度，同时利用聚乳酸的支架性能，构建BMP-2/PLA涂层，通过PLA自身降解调节BMP-2的缓慢释放，促进种植体与周围骨组织的早期骨愈合。BMP-2/PLA涂层表面不断更新，组织细胞粘附生长，促进种植体与周围骨组织的整合，缩短治疗周期。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明，但不以任何方式限制本发明。下述实施例中，如无特殊说明，所使用的实验方法均为常规方法，所用试剂等均可从化学公司购买。
实施例1
一种具有BMP/PLA缓释复合涂层的种植体活性表面，所述种植体外表面具有钛基底层，所述钛基底层外表面具有二氧化钛基层，所述二氧化钛基层的外表面涂覆有BMP/PLA复合涂层，按照如下方法制备得到：
(1)将钛金属种植体表面用200、300、600和2000目砂纸逐级打磨，清洗，在60℃烘干；
(2)用75μmTiO2颗粒，通过喷嘴对种植体表面进行喷砂处理，所述的喷砂处理条件为：压缩空气压力为0.3-0.4MPa，喷嘴离种植体表面的距离为5cm，喷射时间为5s；
(3)将喷砂处理后的种植体置于氢氟酸与盐酸组成的混合酸蚀剂中进行表面刻蚀处理，刻蚀处理温度为60℃，刻蚀处理时间为10min，取出种植体超声清洗，室温自然干燥；
(4)将进行表面刻蚀处理、干燥后的种植体置于60℃、5mol/L NaOH溶液孵育24h，用水超声清洗后，干燥后600℃下处理1h；
(5)将高温处理后的种植体在紫外线下消毒24h；
(6)将聚乳酸溶于CH3Cl3，加入蒸馏水制成乳化液，将步骤(5)中紫外线消毒好的种植体，在无菌条件下浸入聚乳酸乳化液中，置于通风处蒸发水和溶剂，重复上述操作数次，得聚乳酸涂层种植体；
(7)聚乳酸涂层种植体浸入1mg/mL BMP-2溶液中，在4℃下放置24h，真空冷冻干燥，每隔12小时换液一次；
其中，在步骤(3)中，所述的混合酸蚀剂为47％的HF与38％的HCl以体积比1:1混合的混合液；在步骤(7)中将BMP-2溶解于pH值为7.0的SBP溶液中，得BMP-2溶液。
复合涂层的厚度为10.8μm，用ELISA法检测复合涂层体外释出BMP-2的量，测定结果显示，涂层在PBS溶液中浸泡4周后，释放出了总重量的75％。
实施例2
一种具有BMP/PLA缓释复合涂层的种植体活性表面，所述种植体外表面具有钛基底层，所述钛基底层外表面具有二氧化钛基层，所述二氧化钛基层的外表面涂覆有BMP/PLA复合涂层，按照如下方法制备得到：
(1)将钛金属种植体表面用200、300、600和2000目砂纸逐级打磨，清洗，在60℃烘干；
(2)用75μmTiO2颗粒，通过喷嘴对种植体表面进行喷砂处理，所述的喷砂处理条件为：压缩空气压力为0.3-0.4MPa，喷嘴离种植体表面的距离为10cm，喷射时间为10s；
(3)将喷砂处理好的种植体置于氢氟酸与盐酸组成的混合酸蚀剂中进行表面刻蚀处理，刻蚀处理温度为60℃，刻蚀处理时间为20min，取出种植体超声清洗，室温自然干燥；
(4)将进行表面刻蚀处理、干燥后的种植体置于60℃、5mol/L NaOH溶液孵育48h，用水超声清洗后，干燥后600℃下处理1h；
(5)将高温处理后的种植体在紫外线下消毒48h；
(6)将聚乳酸溶于CH3Cl3，加入蒸馏水制成乳化液，将步骤(5)中紫外线消毒好的种植体，在无菌条件下浸入聚乳酸乳化液中，置于通风处蒸发水和溶剂，重复上述操作数次，得聚乳酸涂层种植体；
(7)聚乳酸涂层种植体浸入3mg/mL BMP-2溶液中，在4℃下放置48h，真空冷冻干燥，每隔12小时换BMP-2溶液一次；
其中，其中，在步骤(3)中，所述的混合酸蚀剂为47％的HF与38％的HCl以体积比1:1混合的混合液；在步骤(7)中将BMP-2溶解于pH值为7.0的PBS缓冲液中。
复合涂层的厚度为12.1μm，用ELISA法检测复合涂层体外释出BMP-2的量，测定结果显示，涂层在PBS溶液中浸泡4周后，释放出了总重量的80％。

Claims (7)

1.一种具有BMP/PLA缓释复合涂层的种植体活性表面，其特征在于，所述种植体外表面具有钛基底层，所述钛基底层外表面具有二氧化钛基层，所述二氧化钛基层上涂覆有BMP/PLA复合涂层。
2.根据权利要求1所述的种植体活性表面，其特征在于，该种植体活性表面制备方法包括以下步骤：
(1)将钛金属种植体表面用200、300、600和2000目砂纸逐级打磨，清洗，在60℃烘干；
(2)用75μmTiO2颗粒，通过喷嘴对种植体表面进行喷砂处理；
(3)将喷砂处理后的种植体置于氢氟酸与盐酸组成的混合酸蚀剂中进行表面刻蚀处理，取出种植体超声清洗，室温自然干燥；
(4)将进行表面刻蚀处理、干燥后的种植体置于60℃、5mol/L NaOH溶液孵育24-48h，用水超声清洗后，干燥后600℃下处理1-2h；
(5)将高温处理后的种植体在紫外线下消毒24-48h；
(6)将聚乳酸溶于CH3Cl3，加入蒸馏水制成乳化液，将步骤(5)中紫外线消毒好的种植体，在无菌条件下浸入聚乳酸乳化液中，置于通风处蒸发水和溶剂，重复上述操作数次，得聚乳酸涂层种植体；
(7)聚乳酸涂层种植体浸入1-3mg/mL BMP-2溶液中，在4℃下放置24-48h，真空冷冻干燥。
3.根据权利要求1所述的种植体活性表面，其特征在于，在步骤(2)中，所述的喷砂处理条件为：压缩空气压力为0.3-0.4MPa，喷嘴离种植体表面的距离为5-10cm，喷射时间为2-10s。
4.根据权利要求1所述的种植体活性表面，其特征在于，在步骤(3)中，所述的混合酸蚀剂为47％的氢氟酸与38％的盐酸以体积比1:1混合的混合液。
5.根据权利要求1所述的种植体活性表面，其特征在于，在步骤(3)中，所述的表面刻蚀处理温度为60℃，刻蚀处理时间为10-20min。
6.根据权利要求1所述的种植体活性表面，其特征在于，在步骤(7)中，每隔12小时换BMP-2溶液一次。
7.根据权利要求1所述的种植体活性表面，其特征在于，所述BMP-2溶液的制备步骤为：将BMP-2溶解于pH值为7.0的PBS或溶解于SBF溶液中。
CN201611207441.4A 2016-12-23 2016-12-23 具有bmp/pla缓释涂层的种植体活性表面 Pending CN106730040A (zh)

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